Nghiên cứu hệ vật liệu mao quản trung bình chứa kim loại chuyển tiếp: chế tạo, đặc trưng và tính chất xúc tác trong phản ứng oxi hóa một số hợp chất hữu cơ : Đề tài NCKH. QT.08.25

DAI HOC QUOC GIA HA NOI TRl/CJNG DAI HOC KHOA HOC TlT NHIEN DE T A I N G H I E N CLTU K H O A H O C C A P DAI HOC QUOC GIA H A N Q I NGHIEN ClTU HE VAT LIEU MAO QUAN TRUNG BINH CHLTA KIM LOAI CHUYEN Tl£P: CHt TAG, DAC TRl/NG VA TINH CHAT XUC TAG TRONG PHAN ITNG O X I H O A MOT SO HOP CHAT HCTU CO Ma so : QT-08-25 Chii tri de tai : TItS.Nguyen ThiMinh Thir Dr / 2f3Cl Ha Noi - 2008 DAI HOC QUOC GIA HA N O I TRUOfNG DAI HOC KHOA HOC T U NHIEN BAO CAO TOM T A T KET QUA NGHIEN ClTU D £ TAI NGHIEN ClTU KHOA HOC CAP DAI HOC QUOC GIA HA NOI TEN OE TAI: "NGHIEN CUU HE VAT LIEU MAO QUAN TRUNG BINH C H I T A KIM LOAI CHUYEN TIEP: CHE TAO, DAC TRUNG VA TINH CHAT XUC TAC TRONG PHAN iTNG OXI HOA M O T SO HOP CHAT HU U CO" Ma so : QT-08-25 Chii tri de tai : ThS Nguyen ThiMinh Thiv CAC CAN BO THAM GIA: CN Do Hong Quan KTV.Dang Van Long HVCH Le Thj Dung Ha Noi - 2008 BAG CAO TOM TAT KET QUA CUA D £ TAI NGHIEN ClfV CAP DAI HOC QUOC GIA HA NOI QT-08-25 l.TIn de tai: **Nghien ciru he vat lieu mao qudn trung binh chira kirn loai chuyen tiep: Che tao, dac trirng va tinh chatxuc tdc phdn irng oxi hod mot so hop chat hiru ca " Ma so: QT-08-25 2.Chu tri d6 tai: NCS, ThS, Nguyin ThiMinh Thw 3.Cac can bo tham gia: - CA' Do Hong Qudn - KTV, Dang Van Long - HVCHXe Thi Dung Muc tieu va noi dung nghien ciru: 4,L Muc tieu nghien ciru: Hien nay, cacbohidrat dugc xem la nguon nguyen lieu ciia tuang lai, dong vai tro quyet dinh xay dung nen cong nghiep Hoa hoc Xanh - Green Chemistry Thco du bao, den nam 2030 nguyen lieu c6 nguon goc cacbohidrat se thay the 20% nhien lieu va 25% hoa chat tinh vi tu cac nguon nguNcn lieu hoa thach [61] Dieu gop phan dang ke lam giam sue ep ciia toe dp phat trien nhanh chong doi voi an ninh nhien - nguyen lieu tuang lai Glucoza la mot so cac cacbohidrat bien nhat va hien dang la doi tugng nghien ciru cho nhieu qua trinh chuyen hoa tao cac san pham c6 tinh ung dung thuc te Hai duong chuyen hoa dugc quan tam bao gom: hydro hoa va oxi hoa dieu che San pham cua cac qua trinh nay: axit gluconic, glucaric, sorbitol, axit L-ascorbic (vitamin C), c6 nhieu gia tri ung dung doi song, dac biet la thirc pham va dugc pham Viec nghien cuu cac qua trinh tren he xuc tac di th^ dang la mot xu hucVng mai nghien cuu bai nhtrng uu diem \ugt trpi \k dp chpn Ipc san pham an toan kha nang tach loai \ a dieu khicn qua trinh dupe thuc hien mpi each thuan lai han Muc tieu cua de tai la' Tong hop cac he xuc tac mao quan trung binh chua kim loai chuyen tiep kich thuoc nano: Pt,Au c6 hieu qua cho phan ung oxi hoa chpn Ipc glucoza tao axit gluconic Nghien cuu tim cac dieu kien phan ung: nhiet dp thai gian pH, .nham dat dp chpn Ipc axit gluconic cao 4.2,Ndi dung nghien ciru: - Tong hop cac he vat lieu nen MCM-41, SBA-15, SiO: v6 dinh hinh -Phan tan cac kim loai Au, Pt nano tren cac vat lieu nen - Dac trung cac he vat lieu tong hop dupe bang cac phuang phap vat ly va hoa ly hien dai: XRD SEM, TEM, H.-TPR, BET - Nghien cuu qua trinh oxi hoa glucoza tren cac he xuc tac nham dat dp chpn Ipc vai axit gluconic cao San pham phan ung dupe phan tich bang cac phuang phap: sac ky long-khoi (LC-MS) va sac ky long hieu nang cao (HP-LC) Cac ket qua nghien cuu da dat duac SJ.Nghien cuu co' bdn: - Da tong hap dupe cac he vat lieu MCM-41, SBA-15, SiOi v6 dinh hinh Pt/MCM-41, Pt/SBA-15, Pt/Si02 v6 dinh hinh, Au/MCM-41, Au/SBA-15 va Au/Si02 v6 dinh hinh - Da dac trung cac he vat lieu tong hgp dupe bang cac phuang phap vat ly va hoa ly hien dai: XRD SEM TEM H.-TPR BET - Nghien cuu qua trinh oxi hoa glucoza tren cac he xuc tac t6ng hop dupe Kct qua cho tha\' he nen mao quan MCM-41 thich hgp cho phan ung Xuc tac Au va Pt deu cho hieu qua cao song tren xiic tac Au dp chpn Ipc gluconic axit gan nhu tu}'et doi va nhiet dp phan ung giam nhieu so vai xuc tac chua Pt 5.3, Cac san pham khoa hoc: - Da cong bo 02 cong trinh khoa hpc: 01 Bai bao dang tren Tap chi Hoa hpc va 01 bao cao khoa hpc tai Hoi nghi Hoi nghi khoa hpc cua Tru'ang DHKHTN nam 2008 5.4 Ket qua diio tao: - Tham gia Muang dan 03 sinh vien nghien cuu khoa hpc - Ciop phan cho luan an nghien cuu sinh cua chinh tac eia Tinh hinh kinh phi cua de tai: Kinh phidwctc cap: 20 trieu dong Cac chi phi nhw sau: 1- Hoa chat, dung cu : 2- Thue khoan chuyen mon : 3- Van phong pham in an tai lieu : 10,0 trieu 6,2 trieu 4- Hoi thao : 0.9 trieu 1.3 trieu 5- Chi phi khac : 1.6 trieu Cong KHOA QUAN LY 20 trieu Hd noi, ngdy jVthdngJZ^ndm 2008 Chii tri de tai %ti PGS.TS Nfuyln Van Noi ThS Nguyen Thi Minh Thu TRUONG DAI HOC KHOA HOC TU NHIEN MIEU T R U O M G OGSJS.^dw^M^/^^i^m SUMMARIZE REPORT OF THE PROJECT OF VIETNAM NATIONAL UNIVERSITY HANOI l.Title: Study the mesoporous materials containing transitive metals (Pt Au): Synthesis, characterization and catalytic properties of these materials in selective oxidation of glucose 2.Code: QT-08-25 Person of project: Nguyen Thi Minh Thu Key implementers: Nguyen Thi Minh Thu Director Do Hong Quan Implementer Dang van Long Implementer 4.Le Thi Dung Implementer The tagets and the contents of study of the project: - Syntherizing the material systems Pt/MCM-41 Pt/SBA-15,Au/MCM-41, Au/SBA-15 - Characterizing those material systems by methods: XRD Raman H:TPR TEM BET - Studying cataUtic properties of those materials in selective oxidation of glucose Main results: -Results in science: + The supportable materials MCM-41 SBA-15 were synthesized and characterized + Dispered nano size Au and Pt on supportable materials, characterized bv chemi-physico techniques: XRD Raman H2-TPR TEM, BET - Studied the cataKtic properties of the material s\'stems in selective oxidation of glucose The rcsuhs showed that the both of gold and platinic catalyst are effective catalyst for oxidation glucose The conversion of glucose and the selection of gluconic acid are high (>90%) -Results in training: Three students have been trained •Publication: Two reseach papers have been publiched Hanoi, December 2008 Person of project ^ ^ Nguyen Thi Minh Thu DAI HOC QUOC GIA HA NOI TRUONG DAI HOC KHOA HOC TU NHIEN BAO CAO TOAN VAN KET QUA NGHIEN ClTU DE TAI NGHIEN ClTU KHOA HOC CAP DAI HOC QUOC GIA HA NOI TEN DE TAI: "NGHIEN CUU HE VAT LIEU MAO QUAN TRUNG BINH C H I T A KIM LOAI CHUYEN TIEP: CHE TAO, DAC TRUNG VA TINH CHAT XUC TAC TRONG PHAN iTNG OXI HOA M O T SO HOP CHAT HLTU CO" Ma so : QT-08-25 Chii tri de tai : ThS Nguyen Thi Minh Thw CAC CAN BO THAM GIA: CN Do Hong Quan KTV.Dang Van Long HVCH Le Thj Dung Ha Noi - 2008 MUC LUC Trang M DAU I TONG QUAN II MUC TIEU vA NOI DUNG NGHIEN CUXJ CUA DE T A I III PHUONG P H A P NGHIEN ClTU IV CAC KET QUA NGHIEN CUtJ vA 16 16 THAO LUAN 17 4.1 Tong hap vat lieu xuc tac 17 4.1.1 Tong hop vat lieu nen Si02 17 4.1.2 Tong hgp vat lieu nen MCM-41 18 4.1.3 T6ng hgp vat lieu nen SBA-15 19 4.1.4.T6ng hgp vat lieu xuc tac chua nano Pt va dac trung 18 4.1.5.Tong hgp vat lieu xiic tac chua nano Au va dac trung 25 4.2 Nghien ciru phan irng oxi hoa glucozc 30 4.2.1 Nghien ciru phan irng oxi hoa glucoza tren cac he xuc tac chira Pt 30 4.2.2.Nghien cuu phan irng oxi hoa glucoza tren cac he xiic tac chiia Au 35 V.KETtUPilN 45 VI TAI LIEU THAM PHU LUC KHAO • 46 47 MO DAU Vai muc tieu tim ki6m ngu6n nguyen lieu hoa hoc mai tung buac thay the dan cac nguon nguyen lieu hoa thach khong tai sinh, cac qua trinh chuyen hoa cacbonhydrat san pham ung dung la van de dugc nhieu nha nghien cuu va cac to chuc khoa hoc quan tam Ngay tii thap ky 90 the ky XX, cac hang Hoa dau va Hoa chSt nhu: Dow Chemical, OUP, Shell, Mobile-Oil da dau tu nghien cuu nham xay dung cong nghe cac qua trinh san xuat Hoa chat tinh vi tir nguon nguyen lieu cacbohidrat v6 tan [1,2,15] Cho den nay, cacbohidrat dugc xem la nguon nguyen lieu cua tuang lai, dong vai tro quyet djnh xay dung nen cong nghiep Hoa hoc Xanh - Green Chemistry Theo du bao, den nam 2030, nguyen lieu c6 nguon goc cacbohidrat se thay the 20% nhien lieu va 25% hoa chat tinh vi tu cac nguon nguyen lieu hoa thach [20] Dieu gop phan dang ke lam giam sue ep ciia toe phat trien nhanh chong doi vai an ninh nhien - nguyen lieu tuang lai Glucoza la mot so cac cacbohidrat bien nhat va hien dang la doi tugng nghien cuu cho nhieu qua trinh chuyen hoa tao cac san pham c6 tinh ung dung thuc te Hai duong chuyen hoa dugc quan tam bao gom: hydro hoa va oxi hoa dieu che Tren quy mo cong nghiep, dai dien cua phuang phap chuyen hoa bang duong khu hoa la cong nghe san xuat sorbitol, axit L-ascorbic (vitamin C) Trong do, qua trinh oxi hoa dieu che tao san pham axit D-gluconic la mot nhiing qua trinh cong nghiep Ion hien [10,30] Lugng tieu thu axit D-gluconic chii yeu cho ITnh vuc dugc pham va hoa cliat tren thj truong the gioi hang nam khoang 100.000 tan Trong do, phan Ian thu dugc tu qua trinh oxi hoa sinh hoc vai tac nhan enzym [34] Vai qua trinh enzym, quy trinh cong nghe doi hoi dieu kien khiem ngat, trai qua nhieu cong doan nhu phan tach enzym, tach nuac [6,13] Do nhung han che tren cua cong nghe enzym, mot xu huang mai cho qua trinh oxi hoa dieu che axit gluconic la di the hoa xiic tac Xiic tac di the mang nhieu uu diem vugt trgi ve chon loc san pham, an toan, kha nang tach loai va dieu khien qua trinh dugc thuc hien mot each thuan Igi han Neu nhu Pt (Z=78) hay Ir (Z= 77) da dugc biet den nhu la nhung kim loai c6 boat tinh xiic tac manh me thi Au (Z= 79) lai dugc cho la kim loai tro khong c6 boat tinh xiic tac theo quan niem hoa hoc c6 dien Tuy nhien, thai gian gan day, quan diem da hoan toan thay doi bai cac kham pha ve tinh chat xiic tac ky dieu cua kim loai Au cong bo bai Haruta va cac cong su [8,9,10] Theo do, boat tinh xiic tac va trang thai kich thuoc ciia cac hat Au c6 moi lien quan chat che voi Hien nay, xiic tac kim loai Au tro xu hircmg moi ciia ITnh vuc xuc tac di the Nhieu qua trinh chuyen hoa tren co so xiic tac kim loai Au da dugc nghien cuu nhu: phan ling oxi hoa CO, epoxi hoa propylen, hydro hoa metanol tao focmandehit Nam 2002, Biella va cong sir Ian dau tien nghien ciru phan ling oxi hoa dieu che axit gluconic tu D-glucozo tren xiic tac kim loai Au [21 35] Xiic tac kim loai Au cho qua trinh dieu che axit gluconic tu D-gluoczo dugc danh gia la 19 Mot s6 dac diem sinh hgc cua hai loai vi tao bien Iseehrysis galabana va Nannochloropsis oculata phan lap tai Viet Nam 98 Ngo Thi Hodi Thu, Luu Thi Tam vd Dang Diem Hong 20 Xac dinh phan ciia qua trinh oxi hoa Glucozo bang phuong phap s k ky lone (HPLC-UVD, HPLC-RID, LC-MS) 105 Nguyen Thi Minh Thu, Giang Thi Pliuang Ly, Ngo Thi Thuan, Trdn Thi Nhu Mai 21 Nghien cihi xir ly phenol bang H2O2 duoi tac dung hoat hoa cua cua phuc Co(n) - axit xitric 111 Study on decomposition phenol by H2O2 under catalytic action of the complex Co(II) - citric acid Nguyen Vdn Duong, Trdn Thi Mai, Nguyen Vdn Xuyeh 22 Xac dinh vi lugng coban dat va thuc vat bang phuong phap dong hgc xiic tac 117 Microdetermination of cobalt in soil and in vegetable by kinetic - catalytic method Nguyen Vdn Dudtig, Trdn Thi Mai, Nguyen Vdn Xuyeh 23 Nghien cihi ung dung ky thuat chiet pha rin va phuong phap ph6 hap thu nguyen tir hoa hoi lanh de tach, lam giau va xac dinh lugng vet sieu thiiy ngan nuoc 124 Nguyen Xudn Trung, Vu Vdn Tuan, Pham Hong Qudn, Ta Thi Tfido 24 Nghien cuu ung dung phuong phap dong hgc - huynh quang xac dinh lugng vet asen mau nu6c 129 Kinetic fluorometric determination of trace amount of arsenic in water samples II - Xac dinh tong ham lugng asen v6 co dua tren hieu iing dap tat huynh quang murexit bang Cr(VI) II - Determination of total amount of inorganic arsenic based on the quenching effect of murexit in the present of Cr(VI) Chu Xudn Anh, Tg Thi Thdo, Nguyen Thi Hdng My 25 Chiet xuat va nghien curu kha nang oxi hoa dien hoa cua (-)-epigallocatechin (EGC) che xanh Thai Nguyen 134 Extraction and electrochemical oxidation study of EGC from Thai Nguyen green tea Pham Vdn Khang, Dd Dinh Rang, Le Xitdn Que 26 Nghien cuu phan lap cac diterpenoit co hoat tinh sinh hgc tu cay xuyen tam lien {Andrographis paniculata (Burm P.) Njees, Acanthaceae) d mien B k Viet Nam 140 Study on the isolation of biologically active deterpenoids from Andrographis paniculata (Burm F.) Nees, (Acanthaceae) cultivated in northern Vietnam Phan Minh Giang, Dang Bdch Tdi, Nguyen Thi Thai, Phan Tong San 27 Thanh phan hoa hgc va hoat tinh sinh hgc cua tinh dau nghe den {Curcuma zedoaria Rose.) Viet Nam 147 iii Chemical constituents and biological activity of the essential oil from zedoaria Rose, growing in Vietnam Curcuma Le Thi Anh Ddo Nguyen Tuan Anh Nguyen A/ili Tuan, Trinh Tin Nga 28 Mot so phdn hoa hpc cay nghe doc {Curcuma aromatica Xuan Van - Tuyen Quang Some chemical constituents from Rhizome of Curcuma aromatica Tuyen Quang province Salisb.) a huyen 151 Salisb growing in Le Tin Anii Ddo \'u Quae Trung, Nguyen Tuan Anh 29 Nghien cuu phan hoa hoc cay Quyen ba truang sinh Selaginella Beauv spring Study on chemical constituents Selaginella tamariscina tamariscina 156 Beauv spring Le Minli Hd, Dd Tin Thanh Huyen 30 Cac hap chat flavonoit glycosit {La:ierstroetnia speciosa (L,.) Pers.) va triterpenoit tu la cay being lang nuac 160 Pining Thanh Huang Nguyen Xudn Tlidng Do Nggc Lieti, Nguyen Xudn Cuang, Phan Vdn Kiem 31 Nghien cihi chat lam kho oxi hoa cho muc in luai ky thuat so 167 i'leparatmn of dryer for digital stencil printing inks lloan'^ I In Kicu Nguvcn, Nguxen Anii u Le \ dn Huytih 32 Phan irng trung \\a\) cacdanol dau \'o liat dieu trcnig san xuat bot ma sat 173 l\)l>'men/ation ol cardanoi from cashew nut shell liquid rinli Vdn Dung }} long hap nghien cuu tinh chat mot so hap chat chua di vong L3,4-oxadiazol tren ca sO andehit xinamic 179 Pham Win Hoan \'u Quoc Trung 34 Cam bien sinh hoc glucose oxidaza (GOx) tren co sa mang nanocompozit: polypyrol/ ong cacbonnano img dung tnnig phan tich ham lucmg glucose 187 Pol\p\[Tole/carbon nano tube nanocomposite GOx biosensor for the analvtical detection of elucose I il Tin llon;.^ An N'^n\e/: Dcdn Due Truow^ Tin Ngoc Lien Tran Dai L am 3-^ Nghien ciru tvmg licfp (^carolcu tir n duong mia bang nam sai Blakc.\lea trispnra trone tluct bi Icii men P>'3 Stiid\ on ^MuhcsiN ot |i-Laiotc[ic tf>>m sugar cane molasses b\ filamentous funnal / ' / \ / ( ( \ , r \ ; // ; \r -y,; m bh Tca^'Ioi, (Ju.in It //,; \ d I hi PliiOfir.' Lliani hu Tina "^ \\ K I M O s ii [,.!•;, lii.Mii: p ^ l x piv,-[i->l th •[•]- [I;M[ NM ^ ^ i o n - J R - \ Lin^ nuriL: d u \ a [ m e n m i l c a c 19S Bai bao gui Hoi nghj khoa hoc Trircmg DHKHTN 2008 CHE TAO XUC TAC Au/MCM-41 CHO PHAN iTNG OXI HOA CHON LOC GLUCOZO PREPARATION OF Au/MCM-41 CATALYSTS FOR SELECTIVE OXIDATION OF GLUCOSE Nguyin ThiMinh Thir, Trdn ThjNhirMai, Ngo Thj Thuan Khoa Hoa hoc, Truang Dai hpc Khoa hpc Tir nhien DHQG Ha Noi Abstract: The gold catalysts based on ordered mesoporous materials were preparation b> the impregnation (Au/MCM-41) using alumina-silicate as a support material and the dilute aqueous solution of HAUCI4 The nano-Au/MCM-41 materials were characterized by TEM, XRD, H2-TPR methods Activity catalysts of these materials in glucose oxidation were investigated The results showed that the nano-Au/MCM-41 is effeclixe catalyst for selective oxidation of glucose I.M6d2u Sir oxi hoa cacbohidrat noi chung va sir oxi hoa glucoza noi rieng la nhirng qua trinh quan trong cong nghiep hoa chat bai san pham ciia cac qua trinh na\ co gia tri ung dung Ian nhieu ITnh vuc nhu duac pham, thuc pham \'a chat ta> rira |2.4| Hien nham tang hieu qua chpn Ipc cua qua trinh mix cCing nhu giam thieu sir nhilm moi truang bai cac san pham phu viec su dung cac he xiic tac dj the trC-n ca so cac kirn loai quy nhu Pt Au Ag dang cang phat trien nham thay the cac tac nhan oxi hoa truyen thdng HNO3, Br^/dung dich dem Vai cac xiic tac di t h i mot nhiing yeu to quan trpng quyet dinh den boat tinh la kich thuac hat Chang han Au kim loai dupe cho rang khong co boat tinh xiic tac song nlu t6n tai a kich thuac nano (2-lOnm) thi lai co boat tinh xiic tac cao cho sir oxi hoa CO nhiet dp thSp [3,5] Dac biet dupe phan tan tren cac chat nen co be mat rieng Ion a kich thuac nano se d§n d^n nhirng hieu ung dac biet v6 hoat tinh xuc tac cho nhieu phan ling hoa hpc Cong trinh la kk qua nghien cuu t6ng hop he xiic tac Au kich thuac nano phan tan tren chdt n l i MCM-41 Tinh chdt xiic tac cua he vat lieu dupe danh gia phan ii'ng oxi hoa chpn Ipc glucoza II.Thuc nghiem LTdng hop vat lieu nano Au/MCM-41 Vat lieu n6n mao quan trung binh MCM-41 dupe tong hop tu nguon tien chat tetraethylorthosilicat (TEOS), su dung chat tao cau triic cetyltrimethylamonibromo (CTMAB) 8g CTMAB dupe hoa tan dung dich etanol, them dung dich NH4OH dSn pH-lO (dung dich 1) Them tu tu dung djch TEOS da hoa tan etanol \ao dung dich 1, khuay manh gia a nhiet dp phong Gel thu dupe dupe Ipc rua being etanol, say kho a 90^C gia va nung a 500^C gia d^ loai bo CTMAB \ a 6n dinh cau triic Au duac phan tan tren MCM-41 bang phuang phap tam Tien chat vang dugc su dung la HAuCU- Luang HAuCU da tinh toan dupe pha loang bang nuac cat (dung djch 2) Them vao dung dich a tren 20ml dung djch polivinylancol 2% va khuay manh Tiep tuc them vao 20ml dung dich ure 0,1M van tiep tuc khuay Ig MCM-41 dugc them vao hon hpp dung dich Sau tien hanh dun hoi luu hon hgp di the na\ a 80V gia Lpc lay san pham ran va rua bang nuac nong den het elo San pham dugc nung a 450^^C gia de loai bo het cac hpp chat hiru ca 2.Dgc tnrng xiic tdc Mau xiic tac dupe dac trung bang phuang phap nhieu xa tia X tren thiet bj Siemens D5005, ong phat tia X b^ng ddng co buac song K^ = 1.54A dien ap 40KV cuang dp ong phat 30mA, goc quel 20 thay doi tu 0-70 * Anh chup h i l i vi dien tu truyen qua ciia mau vat lieu dupe thuc hien tren thiel bi Jeol-Jem 1010, dp phong dai 300.000 - 800.000 l^n, mau dupe chup a hieu the 80kV S.Phdn ling oxi hoa glucozo' Phan irng dupe thirc hien a pha long, tac nhan oxi hoa la oxi khong khi, khoang nhiet dp nghien cuu tu 30-lOO^C phhn san pham phan ung dupe danh gia bang phuang phap she ky long hieu nang cao HPLC-RID xa xac dinh tong lugng axil bang phuang phap chuan pH III.K6t qua va thao luan 3.1.Nghien ciru itac trung bCing cdc phuang phap hod ly Gian d6 nhi^u xa Ro'nghen (Hinh la.b) cho k^t qua kha quan tren gian xuat hiCMi cac pie dac trung cho \at lieu mao quan trung binh trat tu (a vung goc hep 29 = 0.8"-3" ) Sau phan tan Au len vat lieu mao quan trung binh MCM-41 vat lieu \an giir dugc c^u triic mao quan trung binh vai cac pic vung goc hep ngoai khong eon pha la nao khac Theo M Haruta, tren gian d6 nhilu xa tia X dac trung tinh the Au xuat hien a cac vung 20 = 38 44.5 va 64.5 [5] Tuy nhien, tren gian nhieu xa tia X khong iha\ sir xudt hien cua cac pic na> Nhu x a> chiing to cac hat \ ang l6n tai a dang kich ihuac nho kich thuac nano nen khong xuat hien dac trung tren gian nhilu xa Ranghen M^t khac gia tri goc 20 cua pic dac trung dich chuyen vk vung 20 Ian han mot chiit chiing to da CO sir hinh ciia cac hat vang nano mao quan lam cho duang kinh mao quan hep han nen dan den su dich chuyen (a) (b) Hinh 1: Gidn dd nhieu xa tia X cua mdu MCM-41 (a) vd Au/MCM-41 (b) Ket qua chup hien vi dien tu truyen qua (TEM) cua cac mau MCM-41 \a Au MC'M41 dupe dua a hinh 2a va 2b Quan sat tren hinh ta thay \al lieu nen co cau true mao quan luc lang dac trung co dp trat tu va dp dong deu cao Duang kinh mao quan khoang 4,5nm Anh TEM ciia mau Au/MCM-41 xuat hien cac dam mau den sam lii cac hai Au nho hinh mao quan ciia MCM-4 Ham cho mao quan cua \al lieu duong nhu day ho'n Dieu cho thay kich ca cac hat Au hinh nit nho (•' 4.5nm) bi hiit vao mao quan ciia MCM-41 bai lire mao quan (a) it) I Hinh 2: Anh TEM cua mdu MCM-41 (a) vd Au/MCM-41 (h) Y)t CO them nhimg thong tin nham khang dinh su hinh nano Au phan tan mao quan MCM-41 chiing toi da tong hap mau \at lieu A3 theo qu\ trinh long hpp Au/MCM-41 (phAn 2.1) nhung khong su dung chat khu ure (Mau A3) Mau xiie tac nav duac tiln hanh khu hoa hidro theo chirang trinh nhiet dp ( l l r l P R ) (^ua trinh khu dugc tien hanh a nhiet dp 25-700'C Trong vung nhiet dp nav oxit silic (MCM-41) khong bi khu [1,2] Tren gian d6 HrTPR ciia mlu vat lieu A3 (Hinh 3) ehi xudt hien I pic khu nhat a vung nhiet dp khu thdp chirng to Au hinh a kich thuac nho xa rat dong deu Hinh 3: Gidn dd HrTPR cua mdu A3 Nhu vay, vai cac ket qua dac trung XRD, TEM, H2-TPR da chung to su cong viec tong hop vat lieu xiic tac nano Au/MCM-41 Au hinh a kich thuac nho (